Hydrochloric Acid → HCID 86738481, compound

HRID 1759164Notes

Reaction equation

HRID 1759164 reaction equation
[CH3:1][O:2][C:3]([P:7]([CH3:11])(=[O:10])[O:8]C)([O:5][CH3:6])[CH3:4].Cl.[OH-].[Na+:14]>>[CH3:1][O:2][C:3]([P:7]([CH3:11])(=[O:8])[O-:10])([O:5][CH3:6])[CH3:4].[Na+:14]

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 54446102Methyl (1,1-dimethoxyethyl)methylphosphinate

Product 1

HCID 86738481HCID 86738481, compound

Procedure

The phosphinate ester product of Example 16 (220 g) was refluxed 2 hr with aqueous sodium hydroxide (2 N: 660 ml). The cooled solution was taken to pH 7.0 with conc. hydrochloric acid, evaporated in vacuo and the solid residue was triturated with methanol and insoluble material filtered off. The filtrate was again evaporated to dryness, the residue triturated with methanol and further insoluble material filtered off. The filtrate was finally evaporated to dryness, triturated with acetone and filtered to give the title compound (2.9 g) mp 258°-262° C., identical (ir nmr) with the product from Example 17.

Workup

  1. customevaporated in vacuo
  2. customthe solid residue was triturated with methanol and insoluble material
  3. filtrationfiltered off
  4. customThe filtrate was again evaporated to dryness
  5. customthe residue triturated with methanol and further insoluble material
  6. filtrationfiltered off
  7. customThe filtrate was finally evaporated to dryness
  8. customtriturated with acetone
  9. filtrationfiltered

Sources & evidence

ORD record
ord-9cf1218397fa40f99dfc1368acc821ef
Source dataset
uspto-grants-1982_07
Patent number
US04339443

Reaction notes

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